CN115007173B - CuInS 2 Preparation of quantum dot carbon aerogel photocatalyst and application of quantum dot carbon aerogel photocatalyst in synthesis of xylonic acid by photocatalytic oxidation of xylose - Google Patents
CuInS 2 Preparation of quantum dot carbon aerogel photocatalyst and application of quantum dot carbon aerogel photocatalyst in synthesis of xylonic acid by photocatalytic oxidation of xylose Download PDFInfo
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- CN115007173B CN115007173B CN202210617168.1A CN202210617168A CN115007173B CN 115007173 B CN115007173 B CN 115007173B CN 202210617168 A CN202210617168 A CN 202210617168A CN 115007173 B CN115007173 B CN 115007173B
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 71
- 239000004966 Carbon aerogel Substances 0.000 title claims abstract description 54
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 44
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 title claims abstract description 42
- QXKAIJAYHKCRRA-UHFFFAOYSA-N D-lyxonic acid Natural products OCC(O)C(O)C(O)C(O)=O QXKAIJAYHKCRRA-UHFFFAOYSA-N 0.000 title claims abstract description 36
- QXKAIJAYHKCRRA-FLRLBIABSA-N D-xylonic acid Chemical compound OC[C@@H](O)[C@H](O)[C@@H](O)C(O)=O QXKAIJAYHKCRRA-FLRLBIABSA-N 0.000 title claims abstract description 36
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 29
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 title claims abstract description 21
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 230000003647 oxidation Effects 0.000 title description 6
- 238000007254 oxidation reaction Methods 0.000 title description 6
- 230000015572 biosynthetic process Effects 0.000 title description 3
- 238000003786 synthesis reaction Methods 0.000 title description 3
- 239000000243 solution Substances 0.000 claims abstract description 52
- 239000007864 aqueous solution Substances 0.000 claims abstract description 26
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000661 sodium alginate Substances 0.000 claims abstract description 21
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 21
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000010992 reflux Methods 0.000 claims abstract description 16
- 238000000137 annealing Methods 0.000 claims abstract description 13
- 239000012670 alkaline solution Substances 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004108 freeze drying Methods 0.000 claims abstract description 9
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 9
- 238000007146 photocatalysis Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000013032 photocatalytic reaction Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000008367 deionised water Substances 0.000 claims description 28
- 229910021641 deionized water Inorganic materials 0.000 claims description 28
- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 claims description 26
- 108010024636 Glutathione Proteins 0.000 claims description 13
- 229960003180 glutathione Drugs 0.000 claims description 13
- 239000004964 aerogel Substances 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000001509 sodium citrate Substances 0.000 claims description 10
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 10
- 239000012691 Cu precursor Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 6
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 5
- 229910021617 Indium monochloride Inorganic materials 0.000 claims description 5
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical group [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 5
- APHGZSBLRQFRCA-UHFFFAOYSA-M indium(1+);chloride Chemical group [In]Cl APHGZSBLRQFRCA-UHFFFAOYSA-M 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 34
- 238000004519 manufacturing process Methods 0.000 abstract description 20
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 abstract description 17
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 abstract description 17
- 239000000811 xylitol Substances 0.000 abstract description 17
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 abstract description 17
- 229960002675 xylitol Drugs 0.000 abstract description 17
- 235000010447 xylitol Nutrition 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 15
- 238000001914 filtration Methods 0.000 abstract description 11
- 239000000706 filtrate Substances 0.000 abstract description 7
- 238000004064 recycling Methods 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 30
- 238000006243 chemical reaction Methods 0.000 description 23
- 239000000047 product Substances 0.000 description 10
- 230000035484 reaction time Effects 0.000 description 10
- 238000010586 diagram Methods 0.000 description 7
- 238000007789 sealing Methods 0.000 description 7
- 238000003756 stirring Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000005286 illumination Methods 0.000 description 5
- 230000005418 spin wave Effects 0.000 description 5
- 229910052724 xenon Inorganic materials 0.000 description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical class O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 2
- JVKRKMWZYMKVTQ-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]pyrazol-1-yl]-N-(2-oxo-3H-1,3-benzoxazol-6-yl)acetamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C=1C=NN(C=1)CC(=O)NC1=CC2=C(NC(O2)=O)C=C1 JVKRKMWZYMKVTQ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- KZEVSDGEBAJOTK-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[5-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CC=1OC(=NN=1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O KZEVSDGEBAJOTK-UHFFFAOYSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000031018 biological processes and functions Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B01J35/23—
-
- B01J35/39—
-
- B01J35/40—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
- C07C51/23—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of oxygen-containing groups to carboxyl groups
- C07C51/235—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of oxygen-containing groups to carboxyl groups of —CHO groups or primary alcohol groups
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a CuInS 2 Preparation of quantum dot carbon aerogel photocatalyst and application thereof in producing xylonic acid by photocatalysis belong to the technical field of catalysis. The preparation method of the catalyst comprises the following steps: preparing various precursor solutions into CuInS by using a reflux method 2 And dispersing the quantum dots and graphene oxide into a sodium alginate aqueous solution, and freeze-drying and annealing the obtained mixture to obtain the quantum dot. The application process of the catalyst in the photocatalytic production of the xylonic acid is as follows: cuInS is to 2 Mixing a quantum dot carbon aerogel photocatalyst, xylose and an alkaline solution, and carrying out photocatalytic reaction; filtering to remove catalyst, and measuring xylitol content of filtrate by high performance liquid chromatograph. The catalyst prepared by the method has the advantages of high catalytic activity, good stability, recycling and the like, is simple and efficient for catalyzing and producing the xylonic acid, and has good application prospect.
Description
Technical Field
The invention relates to a CuInS 2 Preparation of quantum dot carbon aerogel photocatalyst and application thereof in producing xylonic acid by photocatalysis belong to the technical field of catalysis.
Background
With the increasing exhaustion of non-renewable resources such as petroleum, the production of chemical products from renewable biomass as a raw material has become a trend of realizing sustainable development of the chemical industry. The xylonic acid is an important high-value chemical produced by biomass refining and is mainly used in the fields of food, pharmaceutical industry, adhesives and the like. In society requiring sustainable development, the market for xylonic acid is growing. At present, the main production process of the xylitol is obtained by fermenting hemicellulose hydrolysis xylose by utilizing enzymes. However, the biological process has the defects of low yield, harsh reaction conditions (temperature and pH value), complex microbial population control and the like. Therefore, the development of an efficient and environment-friendly method for synthesizing the xylitol has important significance.
Disclosure of Invention
The invention aims at overcoming the defect of the existing photocatalysis production of xylonic acid and providing a CuInS 2 Preparation method of quantum dot carbon aerogel photocatalyst and application thereof in producing xylonic acid by photocatalysis. The method prepares the CuInS from various precursor solutions by using a reflux method 2 The quantum dot is prepared by dispersing the quantum dot and graphene oxide into sodium alginate aqueous solution, freeze-drying and annealing the obtained mixture to obtain the photocatalyst, and the CuInS is prepared by a simple method 2 Quantum dot carbon aerogel photocatalyst and CuInS 2 The quantum dot carbon aerogel is a photocatalyst, and xylose is converted into xylonic acid through a photocatalytic reaction. The method for preparing the catalyst has universality and can be produced in large scale. The catalyst used in the invention has the advantages of good stability, high catalytic activity, recycling and the like. The synthesis method of the invention is simple and easy to control, low in cost and pollution-free.
In order to achieve the above purpose, the invention adopts the following technical scheme:
CuInS for synthesizing xylonic acid by photocatalytic oxidation of xylose 2 The preparation method of the quantum dot carbon aerogel photocatalyst comprises the following steps:
(1) Dissolving glutathione In deionized water to obtain glutathione solution, adding Cu precursor water solution, in precursor water solution, S precursor water solution and sodium citrate water solution into the glutathione solution, refluxing at 85.0-98.0 ℃ for 15.0-180.0 min, washing, and drying to obtain CuInS 2 A quantum dot; wherein, the ratio of the glutathione to the deionized water is 0.05 g-0.3 g:120.0mL, preferably 0.183g:120.0mL; the concentration of the Cu precursor aqueous solution is 0.001-0.05 mol/L, preferably 0.01mol/L; the concentration of the In precursor aqueous solution is 0.1-2.0 mol/L, preferably 1mol/L; the concentration of the S precursor aqueous solution is 0.5-3.0 mol/L, preferably 2.5mol/L; by a means ofThe concentration of the sodium citrate aqueous solution is 0.1-2.0 mol/L, preferably 1mol/L; the volume ratio of the Cu precursor aqueous solution, the In precursor aqueous solution, the S precursor aqueous solution, the sodium citrate aqueous solution and the deionized water is 3-9: 1 to 4:0.1 to 2:2 to 5:120.0, preferably 6:3:0.744:3:120.0;
(2) CuInS obtained in the step (1) is processed 2 Dispersing quantum dots and graphene oxide into deionized water to form mixed dispersion liquid; wherein the CuInS 2 The proportion of the quantum dots, the graphene oxide and the deionized water is 20-200 mg:100mg:25.0mL, preferably 100mg:100mg:25mL;
(3) Dissolving sodium alginate in deionized water to form sodium alginate solution; wherein the proportion of the sodium alginate to the deionized water is 0.2-0.5 g:25.0mL, preferably 0.2g:25mL;
(4) Mixing the mixed solution obtained in the step (2) with the sodium alginate solution obtained in the step (3), and freeze-drying to obtain aerogel; wherein, the volume ratio of the mixed solution obtained in the step (2) to the sodium alginate solution obtained in the step (3) is 1:1:
(5) Annealing the aerogel obtained in the step (4) in nitrogen atmosphere at the temperature of 350.0-600.0 ℃ for 10.0-30.0 min to obtain CuInS 2 Quantum dot carbon aerogel photocatalyst.
According to the above technical scheme, in the step (1), the Cu precursor solution is preferably CuCl 2 Or Cu (NO) 3 ) 2 The method comprises the steps of carrying out a first treatment on the surface of the The In precursor solution is InCl 3 Or In (NO) 3 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The S precursor solution is Na 2 S, 3-mercaptopropionic acid or thiourea.
According to the above technical solution, in the preferred case, in the step (1), the volume of the Cu precursor aqueous solution is 6.0mL, the volume of the In precursor aqueous solution is 0.3mL, the volume of the S precursor aqueous solution is 0.744mL, the volume of the sodium citrate aqueous solution is 3.0mL, and the volume of the deionized water is 120.0mL.
According to the above technical solution, in the step (1), the reflux temperature is preferably 95.0 ℃ and the reflux time is preferably 60.0min.
According to the above technical solution, in a preferred case, in the step (1), the washing method is as follows: and (3) adding excessive absolute ethyl alcohol into the product obtained in the step (1), and centrifugally washing the obtained suspension.
According to the above technical solution, in the step (1), the drying temperature is preferably 60.0 ℃.
According to the above-mentioned aspect, in the step (1), the drying is preferably further followed by grinding.
According to the above technical solution, in the preferred case, in the step (5), the annealing temperature is 450.0 ℃ and the annealing time is 15.0min.
According to the above technical solution, in the step (5), the annealing is preferably further performed after grinding.
CuInS of the invention 2 The quantum dot carbon aerogel photocatalytic material is characterized by means of X-ray diffraction and the like, and is used as a good photocatalyst to be applied to the synthesis of xylonic acid by photocatalytic oxidation of xylose.
CuInS prepared by the method 2 The application of the quantum dot carbon aerogel photocatalyst in the production of xylonic acid by photocatalytic oxidation of xylose comprises the following reaction processes: the CuInS is prepared by 2 Uniformly mixing the quantum dot carbon aerogel photocatalyst, xylose and alkaline solution, stirring for 30.0min in the dark, and carrying out photocatalytic reaction at 10.0-90.0 ℃ for 15.0-180.0 min; filtering to remove catalyst, and measuring xylitol content of filtrate by high performance liquid chromatograph.
According to the above-described technical scheme, preferably, the alkaline solution is a water-soluble alkaline solution, such as potassium hydroxide solution, sodium hydroxide solution, barium hydroxide solution, sodium carbonate solution, potassium carbonate solution, sodium bicarbonate solution, and the like, and preferably potassium hydroxide solution.
According to the above-described embodiments, the concentration of the alkaline solution is preferably 0.1 to 5.0 mol/L, more preferably 0.1 to 1.0mol/L, and still more preferably 0.2mol/L.
According to the above technical scheme, preferably, the ratio of xylose to alkaline solution to catalyst is 0.04g:4.0mL:2 to 30.0mg, preferably 0.04g:4.0mL:2 to 10.0mg, more preferably 0.04g:4.0mL:4.0mg.
According to the above technical scheme, preferably, the reaction temperature is 60.0 ℃.
According to the above technical scheme, the reaction time is preferably 45.0min.
The CuInS of the invention 2 The application of the quantum dot carbon aerogel photocatalyst in synthesizing xylonic acid by photocatalysis xylose optimizes experimental conditions in the aspects of temperature, reaction time, catalyst dosage, potassium hydroxide concentration and the like; and under optimal reaction conditions (0.04 g xylose, 4.0mL of 0.2mol/L KOH solution, 4.0mg CuInS) 2 Quantum dot carbon aerogel photocatalyst, reaction temperature of 60.0 ℃ and reaction time of 45.0 min) is explored 2 The recycling property of the quantum dot carbon aerogel photocatalyst.
The principle of the invention is as follows:
the CuInS 2 The xylonic acid converted by the quantum dot carbon aerogel photocatalyst can be used as a new energy source and a high-value chemical.
The CuInS prepared by the invention 2 Quantum dot carbon aerogel photocatalysts are used in the photocatalytic production of xylonic acid. CuInS 2 The reaction condition for producing the xylonic acid by the photocatalysis of the quantum dot carbon aerogel is mild. The method has simple process and easily controlled reaction conditions, and the obtained xylonic acid is widely applied to the manufacture of foods, pharmaceutical engineering and adhesives.
The synthesis method of the invention has the following advantages:
(1) The xylitol acid synthesized by the invention is a chemical product with high value, and is an important chemical intermediate;
(2) The preparation method of the catalyst has universality and can be used for large-scale production;
(3) The book is provided withCuInS prepared by the invention 2 The quantum dot carbon aerogel as a catalyst has the advantages of good thermal stability, high catalytic activity, good recyclability and the like;
(4) The method for producing the xylonic acid has the advantages of simplicity, safety, no toxicity, quick response, low energy consumption and the like, and has good application prospect;
(5) The product of the invention provides an effective way for solving the energy crisis problem, and especially provides a brand-new way for refining photocatalytic biomass.
Drawings
FIG. 1 is a view of CuInS 2 XRD spectrum of quantum dot carbon aerogel photocatalyst, wherein a is CuInS with reflux temperature of 95 ℃ obtained after step (3) in example 1 2 Quantum dots, b is CuInS with a reflow temperature of 95 ℃ obtained after step (7) in example 1 2 Quantum dot carbon aerogel catalysts.
FIG. 2 is a graph of temperature versus CuInS for example 4 2 An influence diagram of the photocatalytic production of the xylonic acid by the quantum dot carbon aerogel photocatalyst.
FIG. 3 is a graph showing the concentration of potassium hydroxide versus CuInS for examples 4 and 5 2 An influence diagram of the photocatalytic production of the xylonic acid by the quantum dot carbon aerogel photocatalyst.
FIG. 4 shows the amounts of the catalysts used in example 5 and example 6 versus CuInS 2 An influence diagram of the photocatalytic production of the xylonic acid by the quantum dot carbon aerogel photocatalyst.
FIG. 5 shows the reaction time versus CuInS for examples 6 and 7 2 An influence diagram of the photocatalytic production of the xylonic acid by the quantum dot carbon aerogel photocatalyst.
FIG. 6 is a CuInS of example 8 2 And (3) a catalyst recycling performance diagram for producing xylonic acid by photocatalysis of the quantum dot carbon aerogel photocatalyst.
Detailed Description
The invention will be further illustrated by the following examples for better understanding of technical features of the invention, but the scope of the invention is not limited thereto.
Example 1
(1) Adding 0.183g of glutathione into 120mL of deionized water to obtain glutathione solution, and then adding 6.0mL of 0.01mol/L of CuCl 2 Solution, 0.3mL 1mol/L InCl 3 Solution and 0.744mL of 2.5mol/L Na 2 S solution and 3.0mL of 1.0mol/L sodium citrate solution are added into glutathione solution, and reflux is carried out at 85.0, 90.0 and 95.0 ℃ for 60.0min respectively;
(2) Adding excessive absolute ethyl alcohol into the product obtained in the step (1), and centrifuging the obtained suspension;
(3) Drying the product obtained in the step (2) at the temperature of 60.0 ℃ to obtain CuInS 2 A quantum dot;
(4) 100.0mg of CuInS obtained in step (3) is reacted with 2 Dispersing quantum dots and 100.0mg of graphene oxide into 25.0mL of deionized water to form a mixed dispersion liquid;
(5) Dissolving 0.2g sodium alginate in 25.0mL deionized water to form sodium alginate solution;
(6) Mixing the mixed dispersion liquid obtained in the step (4) and the sodium alginate solution obtained in the step (5), and freeze-drying at-50.0 ℃ for 48.0h to obtain aerogel;
(7) Annealing the aerogel obtained in the step (6) in a nitrogen atmosphere at 450.0 ℃ for 15.0min to obtain CuInS 2 Quantum dot carbon aerogel photocatalyst.
Example 2
(1) 0.183g glutathione was added to 120mL deionized water, followed by 6.0mL CuCl, respectively 2 Solution, 0.3mL InCl 3 Solution and 0.744mL Na 2 S solution and 3.0mL of 1.0mol/L sodium citrate solution were added to 120.0mL of deionized water and refluxed at 95.0℃for different 15.0, 30.0, 45.0, 90.0, 120.0min;
(2) Adding excessive absolute ethyl alcohol into the product obtained in the step (1), and centrifuging the obtained suspension;
(3) Drying the product obtained in the step (2) at the temperature of 60.0 ℃ to obtain CuInS 2 A quantum dot;
(4) 100.0mg of CuInS obtained in step (3) is reacted with 2 Quantum dot and 100.0mg graphene oxide dispersionTo 25.0mL deionized water to form a mixed dispersion;
(5) Dissolving 0.2g sodium alginate in 25.0mL deionized water to form sodium alginate solution;
(6) Mixing the mixed dispersion liquid obtained in the step (4) and the sodium alginate solution obtained in the step (5), and freeze-drying at-50.0 ℃ for 48.0h to obtain aerogel;
(7) Annealing the aerogel obtained in the step (6) in a nitrogen atmosphere at 450.0 ℃ for 15.0min to obtain CuInS 2 Quantum dot carbon aerogel photocatalyst.
Example 3
(1) 0.183g glutathione was added to 120mL deionized water, followed by 6.0mL CuCl, respectively 2 Solution, 0.3mL InCl 3 Solution and 0.744mL Na 2 S solution and 3.0mL of 1.0mol/L sodium citrate solution were added to 120.0mL of deionized water and refluxed at 95.0℃for 60.0min;
(2) Adding excessive absolute ethyl alcohol into the product obtained in the step (1), and centrifuging the obtained suspension;
(3) Drying the product obtained in the step (2) at the temperature of 60.0 ℃ to obtain CuInS 2 A quantum dot;
(4) 100.0mg of CuInS obtained in step (3) is reacted with 2 Dispersing quantum dots and 100.0mg of graphene oxide into 25.0mL of deionized water to form a mixed dispersion liquid;
(5) Dissolving 0.2g sodium alginate in 25.0mL deionized water to form sodium alginate solution;
(6) Mixing the mixed dispersion liquid obtained in the step (4) and the sodium alginate solution obtained in the step (5), and freeze-drying at-50.0 ℃ for 48.0h to obtain aerogel;
(7) Annealing the aerogel obtained in the step (6) in nitrogen atmosphere at 350.0, 400.0, 500.0, 550.0 and 600.0 ℃ for 15.0min respectively to obtain CuInS 2 Quantum dot carbon aerogel photocatalyst.
Example 4
(1) 0.04g of xylose, 4.0mL of potassium hydroxide solution with a concentration of 0.2mol/L and 2.0mg of CuInS prepared in example 1 with a reflux temperature of 95.0℃were taken 2 Quantum dot carbon aerogel lightAdding the catalyst into a pressure-resistant bottle;
(2) Sealing the system in the step (1), adding a magnon, and stirring for 30.0min under dark conditions;
(3) Sealing the system in the step (2), and carrying out illumination reaction for 30.0min at 20.0, 30.0, 40.0, 50.0, 60.0 and 70.0 ℃ by using a xenon lamp light source with the power of 300.0W;
(4) Filtering the system after the reaction in the step (3) to remove the catalyst, and measuring the content of the xylitol in the obtained filtrate by using a high performance liquid chromatograph.
Example 5
(1) 0.04g of xylose, 4.0mL of potassium hydroxide solutions of different concentrations (concentrations of 0.1, 0.3, 0.4, 0.5 and 1.0mol/L, respectively) and 2.0mg of prepared CuInS prepared in example 1 at a reflux temperature of 95.0deg.C were taken 2 Adding the quantum dot carbon aerogel photocatalyst into a pressure-resistant bottle;
(2) Sealing the system in the step (1), adding a magnon, and stirring for 30.0min under dark conditions;
(3) Sealing the system in the step (2), and then carrying out illumination reaction for 30.0min at 60.0 ℃ by using a xenon lamp light source with the power of 300.0W;
(4) Filtering the system after the reaction in the step (3) to remove the catalyst, and measuring the content of the xylitol in the obtained filtrate by using a high performance liquid chromatograph.
Example 6
(1) 0.04g of xylose, 4.0mL of potassium hydroxide solution with concentration of 0.2mol/L and prepared CuInS with reflux temperature of 95.0 ℃ in example 1 with different masses were taken 2 Adding quantum dot carbon aerogel photocatalyst (with mass of 4.0, 6.0, 8.0 and 10.0mg respectively) into a pressure-resistant bottle;
(2) Sealing the system in the step (1), adding a magnon, and stirring for 30.0min under dark conditions;
(3) The system in the step (2) is placed at 60.0 ℃ and is subjected to illumination reaction for 30.0min by using a xenon lamp light source with the power of 300.0W;
(4) Filtering the system after the reaction in the step (3) to remove the catalyst, and measuring the content of the xylitol in the obtained filtrate by using a high performance liquid chromatograph.
Example 7
(1) Taking 0.04g of xylose and 4.0mLPotassium hydroxide solution having a concentration of 0.2mol/L and 4mg of prepared CuInS prepared in example 1 at a reflux temperature of 95.0 ℃ 2 Adding the quantum dot carbon aerogel photocatalyst into a pressure-resistant bottle;
(2) Sealing the system in the step (1), adding a magnon, and stirring for 30.0min under dark conditions;
(3) The system in the step (2) is placed at 60.0 ℃ and is subjected to illumination reaction by using a xenon lamp light source with the power of 300.0W for different time (the time is 45.0, 60.0, 75.0, 90.0 and 120.0min respectively);
(4) Filtering the system after the reaction in the step (3) to remove the catalyst, and measuring the content of the xylitol in the obtained filtrate by using a high performance liquid chromatograph.
Example 8
(1) The CuInS obtained by filtration in example 7 2 After centrifugally filtering the quantum dot carbon aerogel photocatalyst, washing the photocatalyst to be neutral by deionized water, and drying the photocatalyst overnight;
(2) Taking 0.04g of xylose, 4.0mL of potassium hydroxide solution with concentration of 0.2mol/L and 4mg of CuInS obtained in the step (1) 2 Adding the quantum dot carbon aerogel photocatalyst into a pressure-resistant bottle;
(3) Sealing the system in the step (1), adding a magnon, and stirring for 30.0min under dark conditions;
(4) The system in the step (2) is placed at 60.0 ℃ and is subjected to illumination reaction for 45.0min by using a xenon lamp light source with the power of 300.0W;
(5) Filtering the system after the reaction in the step (3) to remove the catalyst, and measuring the content of the xylitol in the obtained filtrate by using a high performance liquid chromatograph;
(6) Filtering the CuInS obtained in the step (5) 2 And (3) centrifugally filtering the quantum dot carbon aerogel photocatalyst, washing with deionized water to be neutral, drying overnight, and repeating the steps (2) - (5) for 10 times.
FIG. 1 is a view of CuInS 2 XRD spectrum of quantum dot carbon aerogel catalyst, wherein a is CuInS prepared in example 2 with reflux time of 60.0min 2 Quantum dot, b is CuInS with a reflux temperature of 95deg.C obtained directly after step (7) in example 1 2 Quantum dot carbon aerogel catalyst, cuInS can be seen from the figure 2 Quantum dotThe spectra of the carbon aerogel catalyst are very similar to those of the unmodified catalyst, and represent CuInS 2 Characteristic peaks of (112), (204) and (312) crystal planes. However, annealed CuInS 2 The XRD spectrum of the quantum dot carbon aerogel catalyst has higher peak intensity and sharper peak shape, which represents that the annealing treatment can obviously improve CuInS 2 Crystallinity of quantum dots.
FIG. 2 is a graph of temperature versus CuInS for example 4 2 An influence diagram of the photocatalytic production of xylonic acid by using the quantum dot carbon aerogel. It was found that with increasing temperature, the xylitol acid yield gradually increased, and reached a maximum when the temperature reached 60 ℃, and decreased when the temperature continued to increase, probably due to the conversion of part of the xylonic acid into other by-products during the reaction.
FIG. 3 shows the alkali concentration versus CuInS in examples 4 and 5 2 The effect of the photocatalytic production of xylonic acid from a quantum dot carbon aerogel is shown in the graph, wherein the concentration of potassium hydroxide in example 5 is 0.1, 0.3, 0.4, 0.5 and 1.0mol/L, the concentration of potassium hydroxide in example 4 is 0.2mol/L, and the reaction temperature is 60.0 ℃. It can be seen that as the potassium hydroxide concentration increases, the xylitol production rate increases and then decreases, reaching a maximum at a potassium hydroxide concentration of 0.2mol/L. This is probably because as the base concentration increases, the concentration of the oxidizing active species increases, and too high a concentration of the oxidizing active species causes oxidative degradation of the xylitol into other byproducts.
FIG. 4 is a graph of the amount of catalyst versus CuInS for example 5 and example 6 2 The effect diagram of the photocatalytic production of xylonic acid by the quantum dot carbon aerogel is shown, wherein the catalyst dosage in the example 6 is 4.0, 6.0, 8.0 and 10.0mg respectively, the concentration of the potassium hydroxide solution in the example 5 is 0.2mol/L, and the catalyst dosage is 2.0 mg. The amount of catalyst is also an important parameter affecting the photocatalytic production of xylonic acid. It was found that the xylitol production rate increased and then decreased with increasing catalyst usage and reached a maximum at 4.0mg. The reason for the reduced yield of xylonic acid may be that scattering and refraction of light caused by the excess catalyst reduces the photocatalytic efficiency of the catalyst.
FIG. 5 is an implementationDifferent reaction time vs CuInS in example 6 and example 7 2 In the graph of the influence of the photocatalytic production of the xylonic acid by the quantum dot carbon aerogel, the reaction time in the example 7 is 45.0, 60.0, 75.0, 90.0 and 120.0min respectively, and the catalyst dosage in the example 6 is set to be 4.0mg and the reaction time is set to be 30.0min. The reaction time has an important effect on the production of xylonic acid by photocatalytic oxidation of xylose. It can be seen from fig. 5 that the yield of xylonic acid increases with increasing reaction time and reaches a maximum at 45.0min. The yield of xylitol was reduced after the reaction time exceeded 45.0min, probably because xylitol was converted to other byproducts as the reaction continued.
FIG. 6 is a CuInS of example 8 2 Catalyst circulation experiments for producing xylonic acid by photocatalysis of quantum dot carbon aerogel photocatalyst. As can be seen from FIG. 6, the conversion of xylose and the yield of xylitol acid remained at high levels after 10 cycles, and the conversion and the yield after 10 cycles were 99.9% and 99.8% of the first cycle, respectively, with little change in reactivity. This indicates CuInS 2 The quantum dot carbon aerogel can still ensure higher catalytic efficiency in the repeated recycling process, and has higher recycling capability and excellent stability.
The foregoing examples are illustrative of part of the practice of the invention, but the invention is not limited to the embodiments, and any other changes, substitutions, combinations, and simplifications that depart from the spirit and principles of the invention are intended to be equivalent thereto and are within the scope of the invention.
Claims (9)
1. CuInS 2 Application of quantum dot carbon aerogel photocatalyst in producing xylonic acid by photocatalysis is characterized in that the CuInS 2 The preparation method of the quantum dot carbon aerogel photocatalyst comprises the following steps:
(1) Dissolving glutathione In deionized water to obtain a glutathione solution, adding a Cu precursor aqueous solution, an In precursor aqueous solution, an S precursor aqueous solution and a sodium citrate aqueous solution into the glutathione solution, and refluxing at 85.0-98.0 ℃ for 15.0-180 DEG C0min, washing, and drying to obtain CuInS 2 A quantum dot;
the ratio of the glutathione to the deionized water is 0.05 g-0.3 g:120 mL; the concentration of the Cu precursor aqueous solution is 0.001-0.05 mol/L; the concentration of the In precursor aqueous solution is 0.1-2.0 mol/L; the concentration of the S precursor aqueous solution is 0.5-3.0 mol/L; the concentration of the sodium citrate aqueous solution is 0.1-2.0 mol/L; the volume ratio of the Cu precursor aqueous solution, the In precursor aqueous solution, the S precursor aqueous solution, the sodium citrate aqueous solution and the deionized water is 3-9: 1-4: 0.1-2: 2-5: 120.0;
(2) CuInS obtained in the step (1) is processed 2 The quantum dots and the graphene oxide are dispersed into deionized water in an ultrasonic manner to form mixed dispersion liquid;
wherein the CuInS 2 The proportion of the quantum dots, the graphene oxide and the deionized water is 20-200 mg:100mg:25.0 mL;
(3) Dissolving sodium alginate in deionized water to form sodium alginate solution;
wherein the proportion of sodium alginate to deionized water is 0.2-0.5 g:25.0 mL;
(4) Mixing the mixed dispersion liquid obtained in the step (2) with the sodium alginate solution obtained in the step (3), and freeze-drying to obtain aerogel;
wherein, the volume ratio of the mixed dispersion liquid obtained in the step (2) to the sodium alginate solution obtained in the step (3) is 1:1:
(5) Annealing the aerogel obtained in the step (4) in a nitrogen atmosphere at 350.0-600.0 ℃ for 10.0-30.0 min to obtain CuInS 2 Quantum dot carbon aerogel photocatalyst.
2. The use according to claim 1, wherein in step (1), the Cu precursor is CuCl 2 Or Cu (NO) 3 ) 2 The In precursor is InCl 3 Or In (NO) 3 ) 3 The S precursor is Na 2 S, 3-mercaptopropionic acid or thiourea.
3. The use according to claim 1, wherein in step (1) the reflux temperature is 95 ℃ and the reflux time is 60.0min.
4. The use according to claim 1, wherein in step (4), the lyophilization conditions are: freeze-drying at-70.0 ℃ for 36.0-48.0 h.
5. The use according to claim 1, wherein in step (5) the annealing temperature is 450.0 ℃ and the annealing time is 15.0min.
6. The use according to claim 1, wherein in step (1), the drying is further followed by grinding.
7. The use according to claim 1, wherein said CuInS 2 The quantum dot carbon aerogel photocatalyst, xylose and alkaline solution are uniformly mixed, and the mixture is subjected to photocatalytic reaction for 15.0-180.0 min at the temperature of 10.0-90.0 ℃.
8. The use according to claim 7, wherein the alkaline solution is a water-soluble alkaline solution, and the concentration of the alkaline solution is 0.1-5.0 mol/L.
9. The use according to claim 7, characterized in that the xylose, alkaline solution, cuInS 2 The proportion of the quantum dot carbon aerogel photocatalyst is 0.04 and g:4.0mL: 2-30.0 mg.
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| CN107201226A (en) * | 2016-03-17 | 2017-09-26 | 上海科技大学 | CuInS2Quantum dot, CuInS2/ ZnS quantum dot and its preparation and application |
| WO2018095442A1 (en) * | 2016-11-22 | 2018-05-31 | 华南农业大学 | Quantum dot and use of composite material thereof in preparing ultraviolet resistant products |
| CN107552072A (en) * | 2017-10-23 | 2018-01-09 | 南昌航空大学 | A kind of graphene CuInS2Nano composite photo-catalyst |
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